HRID2098130

反应详情

EQUATION

反应方程式

HRID 2098130 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a stirring mixture of (E)-ethyl 3-(2-amino-5-(trifluoromethyl)phenyl)acrylate (4 g, 15.4 mmol) in 4N HCl in dioxane (20 mL) was added concentrated HCl (3 mL). The resulting mixture was warmed to 100° C. overnight. The reaction mixture was cooled to rt and then slowly quenched with a cold saturated NaHCO3 solution until pH>7. A normal aqueous extraction with EtOAc was followed. The crude mixture was taken directly to the next reaction without further purification. Retention time(min)=1.849, method [1], MS (ESI) 214.0 (M+H).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to rt
  2. customslowly quenched with a cold saturated NaHCO3 solution until pH>7
  3. extractionA normal aqueous extraction with EtOAc
  4. customThe crude mixture was taken directly to the next reaction without further purification